CN113909481A - Method and device for preparing high-quality gold evaporation material - Google Patents
Method and device for preparing high-quality gold evaporation material Download PDFInfo
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- CN113909481A CN113909481A CN202111182023.5A CN202111182023A CN113909481A CN 113909481 A CN113909481 A CN 113909481A CN 202111182023 A CN202111182023 A CN 202111182023A CN 113909481 A CN113909481 A CN 113909481A
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- crucible
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- cooling liquid
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- purity
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000010931 gold Substances 0.000 title claims abstract description 66
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000001704 evaporation Methods 0.000 title claims abstract description 23
- 230000008020 evaporation Effects 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 23
- 239000000110 cooling liquid Substances 0.000 claims abstract description 34
- 239000012798 spherical particle Substances 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005491 wire drawing Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F2009/0804—Dispersion in or on liquid, other than with sieves
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method and a device for preparing a high-quality gold evaporation material, which are characterized in that high-purity gold 5N is put into a crucible, the crucible is heated to be more than 1064 ℃ to melt the high-purity gold, then a gold melt drops into cooling liquid from a small hole at the bottom of the crucible, and the gold melt is cooled by the cooling liquid to form uniform spherical particles. The invention shortens the preparation flow of the gold evaporation material, reduces the introduction of impurities in the gold processing process and prepares the high-quality gold evaporation material.
Description
Technical Field
The invention relates to the technical field of metal smelting, in particular to a method and a device for preparing a high-quality gold evaporation material.
Background
High-purity gold has the characteristics of low and stable contact resistance, good electrical conductivity and thermal conductivity, easy bonding, easy film formation, good adhesion with a semiconductor substrate and the like, and is an important evaporation coating material in the electronic industry such as integrated circuit devices and semiconductor devices. As large scale integrated circuits are moving toward high speed, small size, narrow pitch, higher demands are placed on the quality of the gold evaporation material. The conventional gold evaporation materials used in production are mostly granular or linear, and the production process route is generally smelting, cleaning, wire drawing, granulating/winding (according to customer requirements), acid washing, water washing and drying. During the smelting and wire drawing processes, secondary pollution such as crucible and residual lubricating liquid is easily caused, so that the impurity elements of C, K, Na and Si in the gold evaporation material are higher, and the product quality of the gold evaporation material is seriously influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method and a device for preparing a high-quality gold evaporation material, which can be used for preparing the high-quality gold evaporation material by shortening the preparation flow of the gold evaporation material and reducing the introduction of impurities in the gold processing process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a high-quality gold evaporation material comprises the following specific steps:
and (3) putting high-purity gold 5N into a crucible, heating to 1064 ℃ or higher to melt the high-purity gold, then dripping the gold melt into cooling liquid from a small hole at the bottom of the crucible, and cooling the gold melt by the cooling liquid to form uniform spherical particles.
Further, the crucible is any one of a tungsten crucible, a high-purity quartz crucible and a high-purity graphite crucible.
Furthermore, the bottom of the crucible is flat or conical, and a small hole with the aperture of 0.5-1.5mm is formed at the bottom of the crucible.
Furthermore, the cooling liquid adopts ultrapure water, and the temperature of the cooling liquid is ensured to be less than or equal to 10 ℃ through a heat exchanger.
Furthermore, nitrogen or argon is used as protective gas in the whole process, and the air pressure is 0.1-0.2 MPa.
The invention also provides a device for realizing the method, which comprises a reaction container, wherein the top of the reaction container is provided with an opening, and the opening is provided with a corresponding cover plate; a crucible is arranged in the upper part of the reaction container, and cooling liquid is loaded in the lower part of the reaction container; one side of the upper part of the reaction container is provided with an air inlet and an air outlet which are used for inputting and outputting protective gas; a product outlet is formed in the bottom of the reaction container; valves are arranged on the air inlet, the air outlet and the product outlet; the induction end of the thermocouple extends into the crucible; and a heating coil is arranged outside the crucible.
Furthermore, an insulation can is fixedly arranged at the upper part of the reaction container, the crucible is arranged in the insulation can, a through hole is arranged at the bottom of the insulation can, and the through hole corresponds to the position of the small hole at the bottom of the crucible.
Furthermore, the device also comprises a heat exchanger, wherein the heat exchanger comprises a refrigerating machine and a heat exchange tube; the heat exchange tube extends into the cooling liquid, an inlet and an outlet of the heat exchange tube are communicated with the refrigerator, and the refrigerator is used for cooling the refrigerating medium in the heat exchange tube after heat exchange with the cooling liquid and outputting the refrigerating medium to the heat exchange tube again to continue to exchange heat with the cooling liquid.
The invention has the beneficial effects that:
(1) the invention innovates the preparation process of the evaporated gold, develops the new preparation process and equipment of the evaporated gold, obtains new process parameters, shortens the preparation process, introduces less impurities of C, Si, K and Na, has good sphericity of the product, no tailing, high purity and good quality;
(2) in the forming process of the invention, the gold loss rate is extremely low;
(3) the new process of the invention has the advantages of short flow, high efficiency, less overstocked flow, fast capital turnover and good benefit.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus in embodiment 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that the present embodiment is based on the technical solution, and the detailed implementation and the specific operation process are provided, but the protection scope of the present invention is not limited to the present embodiment.
Example 1
The embodiment provides a method for preparing a high-quality gold evaporation material, which is used for preparing the high-quality gold evaporation material by adopting a smelting-forming-cleaning-drying process, and has the advantages of short process flow, regular and uniform product shape, less impurity introduction and good product quality. The specific process is as follows:
and (3) putting high-purity gold 5N into a crucible, heating to 1064 ℃ or higher to melt the high-purity gold, then dripping the gold melt into cooling liquid from a small hole at the bottom of the crucible, and cooling the gold melt by the cooling liquid to form uniform spherical particles.
Furthermore, the crucible is any one of a tungsten crucible, a high-purity quartz crucible and a high-purity graphite crucible, the bottom of the crucible is flat or conical, and a small hole with the aperture of 0.5-1.5mm is formed in the bottom of the crucible.
Furthermore, the cooling liquid adopts ultrapure water, and the temperature of the cooling liquid is ensured to be less than or equal to 10 ℃ through a heat exchanger.
Furthermore, nitrogen or argon is used as protective gas in the whole process, and the air pressure is 0.1-0.2 MPa.
Example 2
The present embodiment provides an apparatus for implementing the method described in embodiment 1, as shown in fig. 1, comprising a reaction vessel 100, wherein an opening is provided at the top of the reaction vessel 100, and the opening is configured with a corresponding cover plate 1; a crucible 4 is arranged in the upper part of the reaction vessel 100, and a cooling liquid 7 is loaded in the lower part; one side of the upper part of the reaction vessel 100 is provided with an air inlet 2 and an air outlet 6 for inputting and outputting protective gas; the bottom of the reaction vessel 100 is provided with a product outlet 10; valves are arranged on the air inlet 2, the air outlet 6 and the product outlet 10; the induction end of the thermocouple 5 extends into the crucible 4; the crucible 4 is provided with a heating coil 3 at the outside thereof.
Furthermore, an insulation box 11 is fixedly arranged at the upper part of the reaction container 100, the crucible 4 is arranged in the insulation box 11, a through hole is arranged at the bottom of the insulation box 11, and the through hole corresponds to the position of the small hole at the bottom of the crucible 4.
Further, the device also comprises a heat exchanger, wherein the heat exchanger comprises a refrigerator 8 and a heat exchange tube 9; the heat exchange tube 9 extends into the cooling liquid 7, an inlet and an outlet of the heat exchange tube 9 are communicated with the refrigerator 8, and the refrigerator 8 is used for cooling the refrigerating medium in the heat exchange tube 9 after heat exchange with the cooling liquid 7 and outputting the refrigerating medium to the heat exchange tube 9 again to continue heat exchange with the cooling liquid 7.
Before the reaction, the crucible is put into the heat preservation box through the opening, and the small hole at the bottom of the crucible is opposite to the through hole of the heat preservation box. Then nitrogen or argon is input as protective gas through the gas inlet. The crucible is heated by a heating coil. The finally produced gold particles 12 are output from the product outlet. In the preparation process, a refrigerating machine is used for cooling the refrigerating medium, the refrigerating medium exchanges heat with the cooling liquid through the heat exchange pipe, and the temperature of the cooling liquid is always kept to be less than or equal to 10 ℃.
Example 3
Selecting a tungsten crucible, wherein the aperture of a small hole at the bottom of the crucible is 0.5mm, weighing 100g of 5N high-purity gold, putting the 5N high-purity gold into the crucible, covering a cover plate, vacuumizing, introducing high-purity argon, keeping the air pressure at 0.1Mpa, adjusting the temperature of a cooling liquid to be 2 ℃, heating to 1100 ℃, melting the high-purity gold, dripping the high-purity gold from the small hole at the bottom of the crucible, forming spherical particles with the diameter of 1-1.5mm after the cooling liquid, enabling the particles to be uniform in size and free of tailing, cleaning with ultrapure water, and drying to obtain the high-quality gold evaporation material.
Example 4
Selecting a quartz crucible, wherein the aperture of a small hole at the bottom of the crucible is 1.5mm, weighing 100g of 5N high-purity gold, putting the 5N high-purity gold into the crucible, introducing high-purity argon, controlling the air pressure to be 0.1Mpa, adjusting the temperature of a cooling liquid to be 2 ℃, heating to 1080 ℃, melting the high-purity gold, dripping the high-purity gold from the small hole at the bottom of the crucible, forming spherical particles with the diameter of 5-8mm after the cooling liquid, enabling the particles to be uniform in size and free of tailing, washing with ultrapure water, and drying to obtain the high-quality gold evaporation material.
Example 5
Selecting a quartz crucible, wherein the aperture of a small hole at the bottom of the crucible is 0.9mm, weighing 100g of 5N high-purity gold, putting the 5N high-purity gold into the crucible, introducing high-purity argon, controlling the air pressure to be 0.2Mpa, adjusting the temperature of a cooling liquid to be 5 ℃, heating to 1090 ℃, melting the high-purity gold, dripping the high-purity gold from the small hole at the bottom of the crucible, forming spherical particles with the diameter of 2-3mm after the high-purity gold is cooled, and obtaining the high-quality gold evaporation material after the particles are uniform in size and have no tailing, and are cleaned by ultrapure water and dried.
Example 6
Selecting a tungsten crucible, wherein the aperture of a small hole at the bottom of the crucible is 0.9mm, weighing 100g of 5N high-purity gold, putting the 5N high-purity gold into the crucible, introducing nitrogen, introducing 0.1Mpa under pressure, adjusting the temperature of a cooling liquid to 9 ℃, heating to 1100 ℃, melting the high-purity gold, dripping the high-purity gold from the small hole at the bottom of the crucible, forming spherical particles with the diameter of 2-3mm after the high-purity gold is cooled, and obtaining the high-quality gold evaporation material, wherein the particles are uniform in size and have no tailing, and the high-purity gold evaporation material is cleaned by ultrapure water and dried.
The impurity contents of the high-quality gold evaporant prepared in examples 3 to 6 are shown in table 1. As can be seen from Table 1, the high quality gold evaporant prepared using the methods of examples 3-6 had low impurity levels.
TABLE 1 high purity gold impurity content (ppm)
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.
Claims (8)
1. A method for preparing a high-quality gold evaporation material is characterized by comprising the following specific steps:
and (3) putting high-purity gold 5N into a crucible, heating to 1064 ℃ or higher to melt the high-purity gold, then dripping the gold melt into cooling liquid from a small hole at the bottom of the crucible, and cooling the gold melt by the cooling liquid to form uniform spherical particles.
2. The method according to claim 1, wherein the crucible is any one of a tungsten crucible, a high purity quartz crucible, and a high purity graphite crucible.
3. The method as claimed in claim 1, wherein the bottom of the crucible is flat or conical, and the bottom of the crucible is provided with a small hole having a diameter of 0.5 to 1.5 mm.
4. The method as claimed in claim 1, wherein the cooling liquid is ultrapure water, and the temperature of the cooling liquid is ensured to be less than or equal to 10 ℃ by a heat exchanger.
5. The method of claim 1, wherein nitrogen or argon is used as a shielding gas and the pressure is 0.1-0.2 MPa.
6. An apparatus for carrying out the method according to any one of claims 1 to 5, comprising a reaction vessel having an opening at the top thereof, the opening being provided with a corresponding cover plate; a crucible is arranged in the upper part of the reaction container, and cooling liquid is loaded in the lower part of the reaction container; one side of the upper part of the reaction container is provided with an air inlet and an air outlet which are used for inputting and outputting protective gas; a product outlet is formed in the bottom of the reaction container; valves are arranged on the air inlet, the air outlet and the product outlet; the induction end of the thermocouple extends into the crucible; and a heating coil is arranged outside the crucible.
7. The apparatus of claim 6, wherein an insulation box is fixedly arranged at the upper part of the reaction vessel, the crucible is arranged in the insulation box, a through hole is arranged at the bottom of the insulation box, and the through hole corresponds to the position of the small hole at the bottom of the crucible.
8. The apparatus of claim 6, further comprising a heat exchanger, wherein the heat exchanger comprises a refrigerator and a heat exchange tube; the heat exchange tube extends into the cooling liquid, an inlet and an outlet of the heat exchange tube are communicated with the refrigerator, and the refrigerator is used for cooling the refrigerating medium in the heat exchange tube after heat exchange with the cooling liquid and outputting the refrigerating medium to the heat exchange tube again to continue to exchange heat with the cooling liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111182023.5A CN113909481A (en) | 2021-10-11 | 2021-10-11 | Method and device for preparing high-quality gold evaporation material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111182023.5A CN113909481A (en) | 2021-10-11 | 2021-10-11 | Method and device for preparing high-quality gold evaporation material |
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| Publication Number | Publication Date |
|---|---|
| CN113909481A true CN113909481A (en) | 2022-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111182023.5A Pending CN113909481A (en) | 2021-10-11 | 2021-10-11 | Method and device for preparing high-quality gold evaporation material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200977551Y (en) * | 2006-09-20 | 2007-11-21 | 番禺职业技术学院 | Jewelry alloy granulating device |
| CN101138791A (en) * | 2007-10-16 | 2008-03-12 | 天津大学 | Even-sized particles producing device and method for preparing the same |
| CN101745642A (en) * | 2008-12-08 | 2010-06-23 | 中山骏业佳安特电器有限公司 | Repaired mouth alloy melting granulating method and device for jewelries |
| RU165178U1 (en) * | 2015-04-07 | 2016-10-10 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Казанский национальный исследовательский технический университет им. А.Н. Туполева-КАИ" (КНИТУ-КАИ) | DEVICE FOR CASTING PRODUCTS FROM METALS AND ALLOYS |
| CN107024115A (en) * | 2017-04-27 | 2017-08-08 | 宋佳 | A kind of smelting apparatus and alloy melting method |
| CN208033666U (en) * | 2018-04-13 | 2018-11-02 | 郑州金泉矿冶设备有限公司 | Noble metal vacuum granulator |
-
2021
- 2021-10-11 CN CN202111182023.5A patent/CN113909481A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200977551Y (en) * | 2006-09-20 | 2007-11-21 | 番禺职业技术学院 | Jewelry alloy granulating device |
| CN101138791A (en) * | 2007-10-16 | 2008-03-12 | 天津大学 | Even-sized particles producing device and method for preparing the same |
| CN101745642A (en) * | 2008-12-08 | 2010-06-23 | 中山骏业佳安特电器有限公司 | Repaired mouth alloy melting granulating method and device for jewelries |
| RU165178U1 (en) * | 2015-04-07 | 2016-10-10 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Казанский национальный исследовательский технический университет им. А.Н. Туполева-КАИ" (КНИТУ-КАИ) | DEVICE FOR CASTING PRODUCTS FROM METALS AND ALLOYS |
| CN107024115A (en) * | 2017-04-27 | 2017-08-08 | 宋佳 | A kind of smelting apparatus and alloy melting method |
| CN208033666U (en) * | 2018-04-13 | 2018-11-02 | 郑州金泉矿冶设备有限公司 | Noble metal vacuum granulator |
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Application publication date: 20220111 |